高盐食品基质中总砷测定质控样品制备

Preparation of Quality Control Samples for the Determination of Total Arsenic in High Salt Food Matrices

为构建实验室高盐食品基质中砷含量检测体系和质量控制提供技术支撑,建立高盐基质中总砷测定质控样品的制备方法并进行评价。采用基质加标的方式制备质控样品,分别采用氢化物发生原子荧光光谱(HG-AFS)法和基体匹配-动态反应池技术(DRC)-电感耦合等离子体质谱(ICP-MS)法2种测量方法进行测定,通过随机抽样检验和单因子方差分析以评估样品的均匀性,以t检验法统计分析质控样品的长期稳定性。统计分析结果表明,2种原理不同、准确可靠的测量方法结果之间无显著性差异,质控样品中总砷含量均匀,且在常温下3个月内可稳定保存。分别评估质控样品特性值测量引入的不确定度、瓶间差异引入的不确定度和长期稳定性引入的不确定度,得到带有不确定度报告与表示的特性值。试验建立高盐基体中总砷含量的基体匹配-DRC-ICP-MS测定方法,制备相应的质控样品并进行均匀性检验、稳定性检验和不确定评估,为高盐高基体质控样品制备和评价提供有效可靠的方法和数据参考。

To provide technical support for constructing a arsenic content detection system and quality control in high salt food matrices of laboratory,establish and evaluate a method of preparing quality control samples for the determination of total arsenic in high salt matrices.Quality control samples are prepared by using standard spiking,measured by using hydride generation atomic fluorescence spectroscopy(HG-AFS)and matrix matching-dynamic reaction cell technology(DRC)-inductively coupled plasma mass spectrometry(ICP-MS),respectively.Evaluate the uniformity of samples through random sampling test and one-way analysis of variance,and use t-test method to statistically analyze the long-term stability of quality control samples.The statistical analysis results show that there is no significant difference between the two accurate and reliable measurement methods which with different principles,total arsenic content in the quality control samples is uniform and can be stably stored at room temperature for three months.The uncertainty of quality control samples introduced by the measurement of characteristic values,inter bottle differences,and long-term stability are evaluated,and characteristic values with uncertainty reports and representations are obtained.This study establishes a matrix matching DRC-ICP-MS method for the determination of total arsenic content in high salt matrix,and corresponding quality control samples are prepared and subjected to uniformity testing,stability testing,and uncertainty evaluation,providing an effective and reliable method and data reference for the preparation and evaluation of high salt and high matrix quality control samples.